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Method and device for the sulfonation or sulfation of sulfonatable or sulfatable organic substances and for performing faster, strongly exothermic gas/liquid reactions

a technology of organic substances and sulfonation methods, which is applied in the preparation of sulfuric acid esters, liquid gas reactions of thin-film type, physical/chemical process catalysts, etc., can solve the problems of unsatisfactory product quality, unsatisfactory yield and color of reaction products, and high cost of reactor systems, so as to achieve rapid, highly exothermic gas/liquid reactions

Inactive Publication Date: 2011-06-28
CHEMITHON
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Benefits of technology

One aspect of the disclosure provides a method and device for the sulfonation or sulfation of organic liquid raw materials with an SO3 / air mixture, and for performing rapid, highly exothermic gas / liquid reactions in the conventional thin-layer falling-film reactors, for example, tubular reactors or annular-gap, falling-film reactors (in the form of a double cylinder), characterized by the fact that the feeding of the SO3 / air mixture is distributed to more than one feed location within the reaction tube or of several reaction tubes or in the annular gap of an annular-gap, falling-film reactor, for example two feed locations.

Problems solved by technology

The sulfonation or sulfation reactions are highly exothermic so that, together with high local sulfur trioxide concentrations in the reaction mixture, production of oversulfonated and oversulfated products and undesirable side reactions occur, which have a considerably adverse influence on product quality.
The yield and color of the reaction product are unsatisfactory.
This method does dose the SO3 in two steps, that is, in the first step in a less than stoichiometric amount, but this reactor system is technically expensive and has not found application either.
This leads to local oversulfonation, that is, a large excess of SO3 is offered to the film surface or to the liquid drops that have been formed on the surface.
This leads to undesirable side reactions and to a worsening of the color of the reaction product.
With this method, too, the organic material and the SO3 are brought together simultaneously, as described above, which results in oversulfonation with the disadvantages of side reactions and poor color.
Here too the organic raw material and the SO3 gas are brought together simultaneously, which, because of the local excessive concentration of SO3, results in the occurrence of undesirable side reactions.
Also, the temperature increases greatly because of insufficient removal of heat, which again promotes side reactions and leads to a worsening of the color of the reaction product.
This device has not been used in practice either.
The method has the disadvantage that the product stream is not cooled on the way from the reactor to the cyclone separator (separation of gas / liquid) and therefore the temperature increases greatly.
However, the thickness of the film is not uniform enough, so that uniform sulfonation does not occur.
Besides, the apparatus is too complicated and therefore it has not been applied in practice.
In this method too, the organic raw material and the SO3 are combined simultaneously as described above, which leads to oversulfonation, with the disadvantages of side reactions and poorer color.
Cleaning of the reactor is necessary, which leads to production losses.

Method used

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  • Method and device for the sulfonation or sulfation of sulfonatable or sulfatable organic substances and for performing faster, strongly exothermic gas/liquid reactions
  • Method and device for the sulfonation or sulfation of sulfonatable or sulfatable organic substances and for performing faster, strongly exothermic gas/liquid reactions
  • Method and device for the sulfonation or sulfation of sulfonatable or sulfatable organic substances and for performing faster, strongly exothermic gas/liquid reactions

Examples

Experimental program
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Effect test

example 1

Preparation of Laureth (2EO) Sulfate, Sodium Salt in an Annular-gap Falling-film Reactor According to the Invention

In the embodiment of an annular-gap falling-film reactor according to FIG. 5, a thin-walled (approx. 0.5 mm) double tube (3) having an outside diameter 124.1 mm, inside diameter 116.9 mm, and gap of 2.6 mm was built centered into the annular gap (annular space) (2). The overall tube distance (wall thickness plus gap) was 3.6 mm and the length was 330 mm. The diameter of the reactor (inside diameter of the outer tube(1)) was 5 inches (127 mm) with a reactor length of 1650 mm, with an annular gap (2) width of 6.5 mm, each having a raw material (4) distributor slit (5) on the inner wall (6) of the outer tube (1) and on the outer wall (7) of the inner tube (1) and each with a cooling mantle (14) (see FIG. 5). The diameter of the inner double tube (3) was dimensioned so that the SO3 gas was introduced in an amount of 50% through the annular gap (2) in the upper reaction zone...

example 2

Preparation of Laureth (3EO) Sulfate, Sodium Salt, Liquid in an Annular-gap Falling-film Reactor According to the Invention

In the embodiment of an annular-gap falling-film reactor, a thin-walled double tube with a tube distance (gap) of 3.6 mm and a length of 330 mm was incorporated into the annular gap. The diameter of the reactor was 5 inches (127 mm) with a reactor length of 1650 mm and an annular gap width of 6.5 mm, with one raw material distributor slit each on the inner wall of the outer tube and on the outer wall of the inner tube and each having a cooling mantle (see FIG. 5).

A C12 / 14 fatty alcohol ethoxylate (fatty alcohol=ALFOL C12 / C14, C12 content 51-57%, C14 content 41-47%, molecular weight 196) with 3 mol of ethylene oxide (molecular weight 328, APHA color number=10) were introduced through the two distributor slits in an amount of 297 kg / h (mass flow meter) (=0.906 kmol / h of fatty alcohol ethoxylate) at a temperature of 40° C. uniformly onto the two annular gap surface...

example 3

Preparation of α-olefinsulfonate, Sodium Salt in an Annular-gap Falling-film Reactor According to the Invention

In the embodiment of an annular-gap falling-film reactor, a thin-walled double tube with a tube wall distance (gap) of 6.5 mm and a length of 120 mm was incorporated into the annular gap. The diameter of the reactor was 5 inches (127 mm) and the length was 2 m with an annular gap width of 10 mm, and having one raw material distributor slit each on the inner wall of the outer tube and on the outer wall of the inner tube and each having a cooling mantle (see FIG. 5).

A C12 / 16 α-olefin (C12 max. 2%, C14=62-70%, C16 content 29-37% with a molecular weight of 214, APHA=30) was introduced through the two distributor slits in an amount of 165 kg / h (mass flow meter) (=0.772 kmol / h of α-olefin) at a temperature of 40° C. uniformly onto the two annular gap surfaces. The diameters of the inner double tube were dimensioned so that the 50% of the SO3 gas was introduced through the annular...

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Abstract

A method and a device for the sulfonation or the sulfation of organic liquid raw materials with an SO3 / air mixture and other reaction gases in order to perform rapid, highly exothermic gas-liquid reactions in conventional thin-layer falling-film reactors are disclosed. The introduction of the SO3 / air mixture occurs through several feed locations, which are located within (along) the reaction tube or reaction tubes or in the annular gap of annular-gap falling-film reactors. High peak temperatures, undesirable byproducts, worsening of the color and local oversulfation or oversulfonation, which leads to side reactions, are largely avoided.

Description

BACKGROUND1. Field of the DisclosureThe invention concerns an improved procedure for the sulfation or sulfonation of sulfatable or sulfonatable organic substances and for performing rapid, highly exothermic gas / liquid reactions in conventional thin-layer falling-film reactors, for example, tubular reactors or annular-gap reactors, characterized by the fact that the introduction of the SO3 / air mixture is performed according to the invention through several feed locations within (along) the reaction tube or reaction tubes or in the annular gap of annular-gap falling-film reactors.2. Brief Description of Related TechnologyThe sulfation or sulfonation of organic compounds is carried out according to current methods which consist in reacting the liquid organic starting materials with the gaseous mixtures containing SO3 (for example, with conversion gas, a.k.a. converter gas). The sulfonation or sulfation reactions are highly exothermic so that, together with high local sulfur trioxide co...

Claims

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Application Information

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Patent Type & Authority Patents(United States)
IPC IPC(8): C07C305/00B01J35/02
CPCB01J4/001B01J10/02C07C303/32C07C303/24C07C303/06C07B45/02C07B45/00B01J19/002B01J19/247B01J19/249C07C305/10C07C309/20B01J2219/00094B01J2219/185B01J2219/1943B01J2219/2454B01J2219/2458
Inventor AIGNER, RUDOLFREUNER, HORST
Owner CHEMITHON
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